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Analytical Chemistry Laboratory

Kinectrics’ Analytical Chemistry Laboratory is a specially-equipped chemical analysis facility accredited by SCC for a number of tests, including radiochemical analysis.

Kinectrics performs comprehensive qualitative identification of materials using techniques such as X-ray diffraction, X-ray fluorescence, Fourier Transform infrared spectroscopy and optical microscopy. We utilize a wide range of quantitative equipment including GC-MS, GCs with several different types of detectors, HPLC, ion chromatographs, ICPAES, ICP-MS, uv-vis spectrophotometer.

Our Quality System is backed with Thermo Electron's (formerly Beckman’s) Lab Manager LIMS for sample custody, control, tracking, reporting and audit trail. Specific laboratory capabilities are described as follows:

X-ray diffraction

• Computer-controlled PANalytical X'Pert Pro X-ray diffractometer
• Used for the determination of structural information - hence can specify the form that a material is present as, in addition to chemical composition (e.g. iron oxide is characterized as hematite, magnetite, goethite; carbon present as graphite or diamond)

X-ray fluorescence

• Oxford Ed 2000 X-ray fluorometer with high-resolution detector (136 eV for Mn K_-line)
• With vacuum option for higher sensitivity for low atomic number elements
• Capable of qualitative analyses of solid or liquid samples for Na to U
• Capable of performing quantitative analysis in fixed matrices

Fournier Transform Infrared Spectometers

• Three spectrometers for identification of solids, liquids and gases
• Extensive use for identification of polymers (e.g. identify gasket materials)
• Extensive library search capability both in-house and online
• One instrument dedicated to gas phase work - specifically SF₆ and by-products

Optical microscopes

• A number of optical microscopes covering magnifications from 10x to 1200x
• A Hirox microscope covering magnifications from 50x to 3500x. Special optics allow extra long working distances, enabling the examination of unusually builky samples without sample preparation (hence non-destructive). Shielded work area allows examination of radioactive samples. Built-in digital camera provides automatic image archiving and ready transmisison to clients

Philips XL30 FEG-SEM 

• Secondary and backscattered electron detectors
• EDAX Pheonix embedded EDX Spectroscopy system (new - 133eV resolution) with light element capability and conventional elemental mapping and high spatial resolution elemental mapping capabilities. Hard copy or digital format output available
• Electron Diffraction capability: Orientation Imaging Microscopy (OIM) for grain structure imaging Electron BackScatter Pattern (EBSP) can be used for phase identification

JEOL 2010 TEM-STEM 

• 0.14nm line resolution, 0.25nm point resolution
• Oxford Instrument Link ISIS EDX Spectroscopy system (133eV resolution) with light element capability and high spatial resolution elemental mapping capability
• Hard copy or digital format output
• Low background analytical double-tilt or tilt-rotate holders
• Selected Area Diffraction (SAD) and Convergent Beam Diffraction (CBD)
• High Angle Annular Dark Field (HAADF) imaging in STEM mode
• Digital image acquisition

JEOL 35C SEM

• Oxford Instrument Link ISIS EDX system (133eV resolution) with light element and elemental mapping capability. Hard copy or digital format output

Image Analysis

• Image-Pro Plus software package from Media Cybernetics
• Full function software for processing and analysis of, for example, particle counts, size distribution and shape
• Input either from Polaroid images, TEM negatives via scanner (1200 dpi optical) or directly from optical and electron microscopes

Suitability of instruments and special capabilities

FEG-SEM

The FEG source SEM provides superior performance to conventional W or LaB6 source SEMs. In addition to better ultimate resolution, FEG-SEM provides enhanced performance for situations where chemical analysis of light elements at high spatial resolutions and imaging based on compositional differences are required. Such imaging can be achieved either by the use of backscattered electrons or by high resolution EDX mapping (at >10,000x magnification). The EBSP/OIM system attached to the FEG-SEM also offers the potential of performing structural identification in the SEM

TEM-STEM

The JEOL 2010 TEM/STEM is ideally suited to perform phase identification, combining EDX chemical analysis with electron diffraction. A wide sample tilting range is a particular feature for analysis involving electron diffraction. In addition to standard Selected Area Diffraction (SAD) method, the instrument is optimized for performing micro diffraction methods such as convergent bean electron diffraction (CBED).

Otto Herrmann, 416.207.6000 x6262, otto.herrmann@kinectrics.com